The utility model relates to the technical field of preparation devices, and discloses a cyclopentanone purification preparation device which comprises a device body, a condensation chamber and a stirring assembly, a storage tank is arranged at the bottom of the device body, a supporting base is fixedly connected to the outer portion of the storage tank, and a sealing tank top is arranged at the top of the device body. And a feeding pipe is fixedly connected to the interior of the sealing tank top, the stirring assembly is arranged in the device body, and a condensation chamber is arranged in the device body. Steam in the device body can enter a steam inlet through the formed steam inlet and enter a condensation pipe through the steam inlet, the steam in the condensation pipe is condensed into water drops through cooling liquid in a condensation chamber, the water drops flow into a material storage tank, and therefore integrated purification work can be conducted; the operation process is simpler, the manual intervention is reduced, the operation difficulty and the possibility of errors are reduced, and the overall purification efficiency of the equipment is improved.
The invention belongs to the technical field of fine chemicalengineering and electronic material purification, and particularly relates to a method for efficiently removing trace metal ions (Al, Cr, Cu and Fe) in cyclopentanone by utilizing a chitosan-based adsorbent, so that the trace metal ions reach the electronic-grade purity standard (the total content of the metal ions is 1t; the removal method comprises the following steps: (1) fully mixing the modified chitosan adsorbent with a cyclopentanone solution, and carrying out adsorption for 0.5-20 hours at the adsorption temperature of 20-50 DEG C; (2) separating the adsorbent loaded with the metal ions after adsorption from the cyclopentanone solution to obtain the cyclopentanone solution in which the metal ions are deeply removed and the adsorbent loaded with the metal ions; (3) mixing the adsorbent loaded with the metal ions with a desorption agent for desorption, and then filtering and separating out the adsorbent; and (4) drying the adsorbent, and recycling the adsorbent in the step (1).
The invention discloses a peach ketone synthesis method, which relates to the technical field of essence and perfume synthesis, and comprises the following steps: adding cyclopentanone and glacial acetic acid into a reaction container, starting stirring, adding manganese acetate (II) and cobalt acetate (II), and then adding acetic anhydride; introducing dried air below the liquid level, heating to 80-100 DEG C, dropwise adding D-limonene, and carrying out a heat preservation reaction after dropwise adding is finished; gC monitors the reaction endpoint, and the reaction is stopped when the product purity of the reaction liquid is not increased any more; after the reaction is finished, filtering, carrying out reduced pressure distillation to recover cyclopentanone, glacial acetic acid and unreacted D-limonene, after the recovery is finished, adding methanol and n-heptane into kettle liquid, carrying out water extraction, washing and liquid separation, washing an organic phase with a sodiumbicarbonateaqueous solution, carrying out reduced pressure distillation on the organic phase to recover n-heptane, and after the recovery is finished, obtaining a peach ketone crude product; and carrying out crude drawing and rectification on the peach ketone crude product to obtain a peach ketone finished product. The method has the advantages of mild reaction conditions, low safety risk and few three wastes, and can obtain a high-purity peach ketone finished product.
This invention discloses an alloy catalyst, comprising a support and a copper-rutheniumalloy supported on the support, wherein the copper-rutheniumalloy is: Cu 0.7 Ru 0.3 The alloy catalyst prepared by this invention can be used to prepare cyclopentanone. The catalyst has high activity, good stability, and low price. The reactants used in the reaction are renewable, widely distributed, and inexpensive. The preparation of cyclopentanone using the catalyst of this invention does not require the introduction of acid or alkali, which solves the problem of difficult acid treatment in the prior art. Furthermore, it is not corrosive to the reaction equipment, which is conducive to large-scale production.
The invention belongs to the field of organic synthesis, and discloses a method for realizing selective synthesis of cyano-substituted isoxazoline and 3H-pyrrole-3-ketone through temperature regulation, which comprises the following steps: by taking alkynyl ketoxime as a raw material, coppertrifluoromethanesulfonate as a catalyst and cyanobenzo iodo-oxacyclopentanone (CBX reagent) as a cyanationreagent, reacting at the temperature of 20-50 DEG C under the condition that the temperature is 20-50 DEG C, thereby obtaining the cyano-substituted isoxazoline and 3H-pyrrole-3-ketone with the cyano-substituted isoxazoline and 3H-pyrrole-3-ketone. And carrying out tube sealing reaction in an inert gas atmosphere to obtain the cyano-substituted isoxazoline. When the temperature is increased to 100 DEG C to 120 DEG C, the reaction time is prolonged, and the cyano-substituted 3H-pyrrole-3-ketone is obtained. According to the invention, two different cyano-substituted nitrogen-containing heterocyclic compounds are selectively synthesized through temperature regulation and control and free radical cascade reaction of different paths. The reaction catalyst is less in dosage, the substrate is wide in application range, the operation is simple, and the method is efficient.
This invention discloses an ABS surface scratch repair coating and its preparation method, relating to the field of coating technology. The ABS surface scratch repair coating is prepared by reacting 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane 3,9-dioxide with formic acid to obtain intermediate 1; reacting intermediate 1 with diethyl maleate to obtain intermediate 2; reacting intermediate 2 with ethylenediamine to obtain a polyamino phosphorus-containing curing agent; reacting p-hydroxybenzoic acid with 2-chlorocyclopentanone to obtain cyclopentanone benzoate; reacting nano-cerium dioxide sequentially with 3-chloropropyltrimethoxysilane and cyclopentanone benzoate to obtain modified nano-cerium dioxide; and mixing epoxy resin, polyamino phosphorus-containing curing agent, puerarin, and modified nano-cerium dioxide with acetone as a diluent to obtain the ABS surface scratch repair coating. The ABS surface scratch repair coating prepared by this invention has superior weather resistance and flame retardant properties.
The invention discloses a preparation method of exo-8-oxo-bicyclo [3.2. 1] octane-3-carboxylic acid methyl ester, which comprises the following steps: carrying out deprotonation reaction on cyclopentanone under a strong alkali condition, and then carrying out ortho-alkylation reaction on the deprotonation product and 2-(bromomethyl) methyl acrylate to obtain 2-((2-oxo-cyclopentyl) methyl) methyl acrylate; 2-((2-oxocyclopentyl) methyl) methyl acrylate is subjected to a Michael addition cyclization reaction in a catalyst / organic solventsystem, inner-8-oxobicyclo [3.2. 1] octane-3-carboxylic acid methyl ester is obtained, the reaction continues under the same conditions, and the inner-8-oxobicyclo [3.2. 1] octane-3-carboxylic acid methyl ester is obtained. And carrying out isomerization on the inner-8-oxo-bicyclo [3.2. 1] octane-3-carboxylic acid methyl ester until the inner-8-oxo-bicyclo [3.2. 1] octane-3-carboxylic acid methyl ester is completely converted into the outer-8-oxo-bicyclo [3.2. 1] octane-3-carboxylic acid methyl ester. The preparation method provided by the invention fills up the blank that the ex-8-oxo-bicyclo [3.2. 1] octane-3-carboxylic acid methyl ester cannot be synthesized in the prior art and the extrinsic derivative cannot be synthesized by using the extrinsic raw material in the actual research and development process.
The invention discloses a quinazoline fused benzothiazepine tetracyclic compound serving as a berberine structural analogue, a preparation method of the quinazoline fused benzothiazepine tetracyclic compound and application of the quinazoline fused benzothiazepine tetracyclic compound to preparation of a medicine for treating breast cancer. The structural general formula of the compound is shown as a formula 3, and the compound can be regarded as simulation and optimization of the dominant structure of a natural productberberine. The preparation method of the compound comprises the following steps: taking a benzodithio cyclopentanone compound and a quinazoline-derived dipole compound as raw materials, and carrying out efficient [4 + 3] cyclization reaction in an organic solvent under the action of a phosphinereagent. The method is mild in condition, simple in step, wide in substrate universality, capable of rapidly constructing a compound library containing more than 25 target compounds, and excellent in yield. In-vitro anti-tumor evaluation shows that the compound disclosed by the invention shows remarkable anti-proliferative activity and anti-migration ability to triple negativebreast cancer cells, and has a high selectivity index.
The invention discloses a compound agent for relieving later spring coldness of a wheat pesticide at intervals as well as an application method and application thereof, belongs to the technical field of wheat planting, and aims at solving the technical problem that the effect of an exogenous compound agent for relieving later spring coldness harming the growth of wheat at intervals needs to be further improved in the prior art. The compound preparation specifically comprises methyl 2-pentylcyclopentanone acetate, cholic chloride, an anther accelerant, chelated calcium and water. According to the invention, through a synergistic effect among the components, adverse effects caused by low-temperature adversity can be effectively relieved when the wheat pesticide encounters late spring coldness at intervals, and normal filling and yield formation of grains can be promoted while the cold resistance of plants is improved and the photosynthetic activity is maintained.
The application discloses a preparation method of vitamin C ethyl ether. The preparation method of vitamin C ethyl ether comprises the following steps: S11, reacting vitamin C and cyclopentanone to obtain 5,6-O-cyclopentyl-ascorbic acid; S12, adding chlorosulfoxide dropwise into ethanol to react, then adding 5,6-O-cyclopentyl-ascorbic acid and triethylamine to perform refluxing reaction to obtain 3-O-ethyl-5,6-O-cyclopentyl-ascorbic acidether; S13, reacting 3-O-ethyl-5,6-O-cyclopentyl-ascorbic acid ether with dilute hydrochloric acid to obtain vitamin C ethyl ether; in addition, a solid catalyst is added in step S12. The solid catalyst prepared by a novel method is added in step S12 of the preparation method of vitamin C ethyl ether; the reaction time of step S12 can be shortened to 3-5 hours, and meanwhile, the yield of step S12 can be ensured to reach more than 80%. Compared with the prior art, the method disclosed by the application greatly shortens the reaction time of the core step, which is helpful to improve the production efficiency and further reduce the production cost.
The invention discloses a marking substance for wheat mildewing in winebrewing unprocessed grains and a rapid detection method, which are used for rapidly detecting wheat mildewing on the basis of six scientifically screened marking substances including cyclopentanonemonomer, ethyl 3-hydroxybutyrate, propyl acetate, tert-butyl alcohol, 2-butanone and nonanal, and providing an accurate basis for judging a wheat mildewing stage. Winebrewing raw grain wheat mildew stage division is realized, and wheat mildew detection accuracy is improved. Based on the early-stage mildew marker substance, early-stage detection of wheat mildew is realized, and the detection sensitivity is enhanced; based on the signal intensity and combination characteristics of the marker substance, determining the main mould types of wheat mildew; besides, the rapid detection of the mildew of the wine-making raw grain wheat is verified by multiple methods, and the similarity calculation, dynamic principal component analysis, clustering heat map analysis and voting method or weighted scoring model of mildew samples at different mildew stages are combined, so that the cross validation of the multiple methods is realized; and the accuracy and reliability of determining the mildew stage and the mold type are improved.
The invention discloses bradyrhizobium yuanmingense ASHBWH-23-9 with functions of promoting growth and inhibiting aspergillus flavus and application of the bradyrhizobium yuanmingense ASHBWH-23-9, and the preservation number of the bradyrhizobium yuanmingense ASHBWH-23-9 is CCTCC (China Center for Type Culture Collection) M 20253053. The innovation of the invention lies in that the dual functions of generating cyclopentanone antibacterial volatile matters and efficiently symbiotically fixing nitrogen are integrated in the bradyrhizobium in the circular and clear garden for the first time. The molecular mechanism is that the generated volatile substance can accurately down-regulate the expression of a toxin synthesis key gene and a spore development core gene in aspergillus flavus. Compared with an existing microbial agent with a single function, nodulation and nitrogen fixation promotion and aspergillus flavus inhibition at the source can be synchronously realized at the rhizosphere of the peanuts through one-time inoculation, and particularly, aiming at the characteristics of overground flowering and underground fruiting of the peanuts, the microbial agent continuously plays a role in bacteriostasis and antipoison in soil in the pod development period.
The invention provides a preparation method of furfuryl ketone resin, which comprises the following steps: step 1, mixing furfural, acetophenone, cyclopentanone and furfuryl alcohol according to a mass ratio, and uniformly stirring to obtain a homogeneous mixed solution; step 2, adding a catalyst into the homogeneous-phase mixed solution, and continuously stirring and uniformly dispersing; and step 3, adding the uniformly dispersed solution into a reaction kettle, introducing nitrogen to replace air in the kettle, and carrying out step-by-step temperature control reaction to obtain light yellow to light brown viscous resin liquid. The energy band structure of the bioxometallate is regulated and controlled through rare earth elements, the electrophilic / nucleophilic ability of active sites is enhanced, and generation of C-C bonds is directionally catalyzed; advanced gelation of the resin is inhibited through the polydopamine film; dynamic adaptation of the acid / alkali site proportion is realized by adjusting the doping amount of rare earth, aldol condensation and dehydration crosslinking reaction can be completed in one step, the technological process is simplified, and finally efficient and green synthesis of high-carbon-residue and high-performance furfuryl ketone resin is realized.
The invention discloses a preparation method of non-grain bio-based pentamethylene diamine, and relates to the technical field of bio-based chemical preparation. The preparation method of the non-grain bio-based pentamethylene diamine comprises the following steps: adding furfural and a first catalyst into a first solvent, introducing hydrogen, carrying out a furfuralhydrogenation reaction, and recovering the first catalyst to obtain a reaction liquid of cyclopentanone; adding ammonia water and a second catalyst into the reaction liquid of cyclopentanone, introducing oxygen, carrying out ammoxidation reaction on cyclopentanone, and recovering the second catalyst to obtain a reaction liquid of glutaronitrile; and adding the reaction liquid of the glutaraldehyde and a third catalyst into a second solvent, adding alkali liquor to adjust the pH value to 8-12, introducing hydrogen, carrying out a glutaraldehydehydrogenation reaction, recovering the third catalyst, and carrying out rectification and purification to obtain the pentamethylene diamine. The preparation method disclosed by the invention does not depend on grain raw materials, the process is green and environment-friendly, the catalyst is stable in circulation, and industrial large-scale production and high-purity application scenarios can be met.
Owner:YANGTZE DELTA REGION INST OF TSINGHUA UNIV ZHEJIANG
The invention provides a method for separating cyclopentene and cyclopentane in a C5 component and a preparation method of cyclopentanone, which comprises the following steps: firstly, under the action of a solid acid catalyst, enabling the cyclopentene in the C5 component to react with acetic acid to obtain cyclopentyl acetate, and by virtue of the characteristic that the boiling point difference between ester substances and alkane is relatively large, separating cyclopentene from cyclopentane in the C5 component to obtain cyclopentyl acetate; and separating the cyclopentane from the cyclopentyl acetate to achieve the separation of the cyclopentane and the cyclopentene. Furthermore, cyclopentyl acetate obtained through separation reacts with hydrogen under the action of a hydrogenation catalyst to produce cyclopentanol, cyclopentanol is oxidized under the action of the catalyst and an oxidizing agent to produce cyclopentanone, and unreacted cyclopentanol can be recycled. Through testing, the yield of cyclopentanol is greater than or equal to 90%, the yield of cyclopentanone is greater than or equal to 90%, and the purity of cyclopentane is greater than or equal to 95%.
The application discloses a refining method of cyclopentyl formaldehyde, which comprises the following steps: firstly, reacting the cyclopentyl formaldehyde crude product with a lower alcohol, then reacting with sodiumbisulfite, separating the sulfonatesolid after the reaction, and carrying out a desalting reaction on the sulfonatesolid with potassiumcarbonate to obtain the cyclopentyl formaldehyde fine product. The method improves the separation effect of the cyclopentyl formaldehyde and cyclopentanone, and alcohol is used as the solvent, so that the generated sulfonate is precipitated from the solution, the sulfonate of the cyclopentyl formaldehyde is directly filtered out, and the desalting is carried out with potassiumcarbonate after water is added for cleaning, so that the finished product is generated, the operation is simple, the effect is good, and the yield is high.